Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
40, Number 1, January 2002, pp. 29-34
Simple Determination of 22 Organophosphorous Pesticides in Human
Blood Using Headspace Solid-Phase Microextraction and Gas Chromatography with
Mass Spectrometric Detection
Frank Musshoff*, Heike Junker,
and Burkhard Madea
Institute of Legal Medicine, Rheinische Friedrich-Wilhelms-University, Stiftsplatz
12, D-53111 Bonn, Germany
A simple and rapid procedure for the determination of 22 organophosphorous
pesticides (bromophos-ethyl, bromophos-methyl, chlorfenvinphos, chlorpyriphos,
demethon-S-methylsulfon, diazinon, dichlorvos, dicrotophos, dimethoate, disulfoton,
edifenphos, fenitrothion, fenthion, malathion, methidathion, mevinphos, monocrotophos,
omethoate, parathion-ethyl, parathion-methyl, phosphamidon, and quinalphos)
in human blood using headspace (HS) solid-phase microextraction (SPME) and gas
chromatography (GC)–mass spectrometry (MS) is presented. The effects of
various sample additions, incubation temperatures, absorption times, desorption
times, and depths of fiber insertion into the injection port of the GC are optimized
to enhance the sensitivity of the procedure. The recoveries of spiked blood
samples are determined between 70% and 95% compared with samples prepared in
water, and absolute recoveries are in the range between 0.1% and 19.6%. For
quantitation in the single ion monitoring mode, linearity is established over
concentration ranges from 0.025 to 5.0 µg/g with excellent coefficients
of correlation (0.991–0.998). The detection limits are in the range between
0.01 and 0.3 µg/g. The time for analysis is 44 min per sample including
extraction and GC–MS analysis. HS-SPME in combination with GC–MS is
an effective method for the determination of organophosphorous pesticides in
human blood and shows a great potential for use in rapid on-site analytical
work, which is highly demanded in clinical and forensic toxicology.
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